Purification of oils



Patented Mar. 19, 1929 I UNITED STATES PATENT OFFICE.

EENBY ODEEN, OF PALO ALTO, CALIFORNIA.

runrricarron or OILS.

No Drawing. Application filed July 14, 1926. Serial my. 122,504.

This invention has to do with a process of as well as neutralizing and removing such refining oils and oil emulsions and more parfree fatty acids as are present. ticularly the refining of fatty oils containing It'may be stated at this point that if there free fatty acids, and in its broader aspect is present in the oil, which is rarely the case,

includes the steps of adding to and mixing 'a sufficient amount of water to satisfy the with such oils a finely divided solid mateprocess, or an excess (e. g. if it is desired to rial carrying a dry alkali and adding at any treat an emulsion, i. e'. oil carrying several stage of the process sufficient water to ropercent of water in emulsified condition) mote a rapid neutralization of free atty then it is only necessary to add to subh an loacids and to agglomerate the resultant soap oil the dry chemicalin an amount suflicient stock. to combine with and remove the free fatty one of the more important features of my acids and the other impurities, and the soap invention-resides in the employment in the formed in this reaction will also remove cer-' .process of; a dry reagent or dry chemical ta in excess amounts of water. It is prefer- 15 which-consists of a finely divided solid ma able in such a case, to add such an amount terial carrying a dry substance, such as a of the dry chemical that all the water willdry alkali, capable of acting upon and neube removed from the oil. In its broadest tralizing the free fatty acids of the oil. The aspect my invention, therefore, does not finely divided material may be inert and necessarily contemplate the addition of wa-.

2 non-absorbent and the dry reagent may be ter where a sutficient amount thereof already formed, for example by thoroughly mixing exists in the oil to be refined.- In all cases the inert non-absorbent material in powdered where water is to be added to the fatty oils, form with a concentrated solution of the except where it is desirable ,to leave a coll alkali, such as caustic soda, drying the said ored'oil as in the case of salad oils, I prefer mixture, and grinding or pulverizing the to first add and thoroughly mix the dry.

resulting cake to a relatively fine powder. chemical with the oil to be treated so as to The surfaces'or substantial portions thereof obtain the beneficial results of a previous of the particles of powder will thereforebe scrubbing action upon the oil and thus sea coated with and carry a closel adherent cure a more complete-removal of the color- 30 thin film of dry alkali. This ry powder ing, colloidal, mucilaginous and finely di- 8 5 will hereinafter be referred to, for brevity, vi'ded suspended matters. as dry chemical. So formed'the dry chem- The present invention relates to and n.- ical, when added to the oil, is in an ideal -volves what will herein be termed a dr state or condition not only to remove colorprocess, since, while water is used in t e 3.3 ing, mucilaginous colloidal and finely dioperation, it is practically all absorbed by so vided suspended. matters, but also, when in the reaction products and by the dry chem1- the presence of water, to enable the reaction cal added. In practice the process involves between the alkali and the acid components the use of a limited amount of .water so that of the oil to proceed with avidity. However, it will be within the absorptive capacity of 40 I prefer, for reasons more fully ointed out the reactionproducts, and the use of a dry e n to empl y a finely dlvided solid chemical to produce the reactions and assist material which will absorb and to some exin absorbing the water. The soap is the tent be impregnated with the alkali in the principal reaction product and this together step of forming the dry chemical, and I with the precipitated coloring, colloidal and v r 4- shall describe my invention in detail in finely divided suspended matters are left.

connection with such a finely dividedsolid closely adherent to and entangled withthe' absorbent material impregnated with'a dry residue of the dry chemicalin a substantlally alkali. My process is also applicable to the solid agglomerated state at the conclusion refining of the fatt oils in which a substanof the treatment, whereas in the commercial 5o tial proportion of fatty acids have been preprocesses heretofore generally used 1ndus- .viously removed and in which process the trially, enough water is present so that these alkali carried by the finely divided solid 'soaps'and similar products exlsted as llquld material serves to further purify the oil with solutions at this stage, hence these prior i respect to its coloring, colloidal, mucilagie processes can betermed fwet. processes. It I 55 nous and finely divided suspended matters, is on account of their solid form and due to*- Y to be the preferred embodiment of my in-" the absence of excess water that the said soap products and other impurities are rendered more insoluble in the oil, causing the same to be more readily precipitated and be very easily removed in the entirety from the purified oil in my improved process, and this I consider to be an important achievement. I will now describe 1n detail what- I consider vention; v

The present invention specifically contemplates the use of a dr form of alkali or neutralizing agent (pre erably caustic soda-beadded to the oil during the operation (e. g.

before, during or after the, addition "of the pulverulent material, but not pre-mixed therewith) to aid and hasten the reaction between the alkali and the acid components in the oil, and this addition of water also serves to so 'control said reaction so that the alkali is prevented from saponifying any appreciable amount of neutral oil but is confined to the neutralization of acidity and the removal of other impurities. If no water were added during the process and onl the usual traces of moisturefound in cru e. oils were present, the reaction would beextremely sluggish and would not proceed to completion for a long period of time, but the instant that water makes coninto the operation is so limited as to supply the needs of the process only, and the amount of water added is capable of being absorbed bythe dry reagent added, and the solid reaction products including the soap. By thus controlling the reaction a more nearly quantitative separation of acid components can be effected than by using an excess of aqueous solution of alkali which is the common method employed in the practice of the art. I I

p A slight excess of free water which necessarilywould be present or added during the operation would not be available for the saponification of any substantial amount of neutral oil because of the presence of the dry chemical and reaction products which have. dehydrating properties. The films of soap which are formed in the reaction assist inthe dehydration of the oil after the esmethod in all of its embodiments is that it I will remove more coloring, mucilagin us, colloidal, and finely divided suspended matters existing in the oil before or duringitreatment, than will the ordinary wet neutralizing methods. Thismay be partly due to thecauterizing action of the caustic alkali ex isting in such active state, and in m preferred embodiment paitly due to t e increased insolubility of the reaction products which inhibits distribution of color, and other impurities.

By the use of my method, oil-washing and oil-drying equipment is not needed, and the bleaching equipment can be much simplified, thus lending to, considerable economy in the apparatus used.

f The present invention is broadly applicable to fatty oils in general, including those oils which are solid at normal temperature as well as those oils which are liquid at normal temperature, and the term .oils is intended to cover both normally liquid oils and normally solid oils and fats. The

present application is particularly con-' cerned with liquid fatty oils of animal and vegetable origin; for example, cotton seed oil, corn oil, castor oil, rape oil, soy bean oil, cod liver oil, and various other liquid fish oils, (ormarine oils), lard oil, and,

generally, all liquid fatty oils from which it i is desired to remove the free fatty acids, whether'it is also desired to improve the color of the oils or not. I

The present invention contemplates a distinctively dry process of refining oils, and while water is used, and is important in the process, the absorptive capacity of the absorbent neutralizing agent and reaction products formed -(particularly the soap) is" preferably substantially in excess of the total. amount of water present or added during the process. I

As in my prior application 727,543, filed July 22, 1924, of which the present'case is a continuation in part, fullers earth or other argilaceous' material is generally the preferred absorptive material in the dry chemical used. Other carriers or vehicles such as kieselguhr, vegetable carbon or charcoal,

these materials, notably sodium carbonate,-

might be considered as not inert since they might exercise more or less neutralizing action upon the free fatty acids. The vehicle' obviously should be one which will not destroy the caustic soda added.

As stated, such a dry solid carrier material may comprise a soap, and in this modifi-' cation, I may for instance apply to a concentrated liquid soap or molten soap, a proportion, preferably a large proportion of.

alkali, say caustic alkali, in the form of a hot supersaturated solution or dry caustic alkali (e. gfpot'vdered). This mixture of soap and alkali should be thoroughly mixed to produce a very homogeneous mass, and

allowed to harden say by congealing or drying. The hardened soap-alkali mixture may then be comminuted to a fine degree of subdivision in a suitable type of grinding equipment.

I have above referred to. sodaash as the vehicle, thus .I may add to molten caustic soda an, equal proportion, moreorless, of

soda'ash, and effect a homogeneous mixture,

then 'cool to solidify the mass andgrind to a fine state of ubdiyision. a

As stated, water is employed in the proc-' ess in an amount capable of promoting the reaction between the free fatty acids and the 'dry alkali, and ordinarily relatively pure water (e. g. ordinary tap water) is preferred.

. However, theme of dissolved salts and dissolved substances in' the water is s not. preeluded. Thus it might be advisable to em-' ploy, instead of pure water, solutions of com-' mon salt, aluminum sulphateor borax, or

other substances which may to someextent i precipitate or destroy coloring matter in the oil or which may to a considerable extent assist in.dragging down and precipitating calloidal or suspended matters, or albuminous matters or other gummy or mucilaginous substances present in the oil. Thus a 5 to 10% solution (or a stronger or weaker solution) of any of these salts can be used instead of water, in the above example;

I The amount of water to be used in the process will vary, depending largely upon the quantity of free fatty acids present in the oil. With oils of ordinary free fatty acid" content (say 3 to 7% free fatty acid content) an amountof water equal to 0.5% up to 2% or 2.5% will generally be satisfactory, although somewhat larger amounts than this may be used if desired. In some cases commercial crude fatty oils (say cotton scedoil) frequently contain more or less free fatty acid content than would be used if the oil is low in free fatty acids. Thus 'with a 5% F. F. A. content oil, I may use about 2% of water, and with a 10% F. F. A. content oil, it may be necessary to use as much as 3.5 to,4% of water.

where in the case, are of course based .on the amount of oil.)

The amount of water above stated can be varied between more or less wide limits. .In treating cotton seed oil, for example, the water can be all added before the introduction of the dry chemical, 01' can be added after the addition of the dry chemical, or can be added during the addition of the dry chemical, but separately therefrom. I do not mix the water with the dry chemical and add the said mixture to the oil to be treated, since this would be wasteful, and I would not get the complete results of the process.

Reference was made above to adding water "first, and' later adding the dry chemical.

Thus in producing a salad oil from crude cotton seed oil, containing say 0.2% of water and 0.6% of free fatty acids, I might first add 1% of water to the oil, while wellagitating, to form an emulsion, and then dump in say 1.5% of the dry chemical, continue ,ical used (say fullers earth impregnated with dry caustic soda) should be capable (assisted by the soap formed in the.process) of absorbing considerably more water than the total amount employed or present 'during the process, and under ordinary conditions the amount of the dry chemical to be used 'will depend orrnumerous factors, including the amountof free fattyacids in the oil to be treated, the amount of decolori zation to be effected and the amount of mucilaginous and gummy materials in the oil. For ordinary purposes 2 to 5% (based on the (The percentages stated in this paragraph, and elseion The amount of active neutralizing reagent, say caustic soda,

should preferably be somewhat in excess of the amount which theoretically would be with and neutralizing the total free fatty acids in the oil under treatment if it is desiredto completely remove -such acids.

The dry chemical which I prefer to use is preferably formed by impre nating a'dry inert absorbent material, such as fullers earth or any of those above referred to, with a solution, preferablya highly concentrated solution, of caustic soda, then I dry the so impregnated material, for exam ple in an OVyQlI at a temperature of 200 to 300 or to 4OQS-;F., or, if desired, much higher ten'iperaturesgcan be used. \Vith 100 parts of ordinary fulle1"searth,I may use 130 M factory chemical to use.

* parts of a saturated (say solution of caustic soda. The material is thereafter dried and the. resulting'cake is ground up or' pulverized to a relatively fine powder. In other cases, with 100 parts of fullers earth satisfactory materialshave been prepared when using from 80 to 150 parts of saturated caustic. soda .solution or weaker solutions, containing 1045% NaOI'I, more or less. 4 I

I have referred above to drying the impregnated fullers earth, but it is to be understood thatthis drying does not'have to be complete to the extent of removing every trace of water. The material is preferably driedJsuflicientlyv so that it will readily absorb and" take up water present in or added 'to the oil. 'The term dry will be so un dcrstoodherein, v

Complete impregnationin the manner described, followed by dryilig, gives a satisowever in'. some cases, caustic soda and fullers earth can be well ground and triturated together, 'say in a moi-tan or edge-runner mill. If the mill is open to the atmosphere the caustic will take up more or less moisture from the atmosphere during this step, or some water can be added to the mass before or as above descri during the grinding and'mixing operationf Thus this will give an intimate association andsubstantially an impregnation. This product can be; tdllien dried and powdered,

In practici g the method of oil refining and purification in its preferred form, generally warm-up the oil to a temperatureat which it is freely liquid and at which it has a suflic-iently 'low viscosity to be readi ly treated. Thistemperature will depend necessary for combiningoil a temperature of 90 to 100 F. is very satisfactory. Irrespective of the particular oil, 1 preferably do not heat to over 140 F., at and above which the heat is likely to set the color and otherwise injure fatty oils. The alkali impregnated solid material (or dry chemical) is then added to the oil, -for example by being sifted or sprinkled upon the top of the agitated body of .oil and is preferably agitated during and for some time after this dry chcmical'has been added. The water to be used is preferably added at this stage, and the break will occur after only a few minutes further agitation.= The oil .and materials contained therein are then allowed to settle andsedimentation will occur quite rapidly. Even in a large bulk of oil it will be found that the solid matter will practically all settle out of the oil, within half an hour or an hour, and the clear oil in the upper part of the receptacle can then be passed throughthe filterpress (or other separating device) and sent to storage tanks as refined oil. I call attention to the fact that the sedimentation here referred to may be cgmplete in a half hour or an hour instead of requiring many times this period as is the usual case in wet methods of refining.

Due to the thorough drying or dehydratfiltered refined oil will be found to be very bright and clear and free fromsoap, and

mg action taking place in the process, the

analysis will show practical absence of water therein, or, say usually well below 0.25%-

to. Theremaining solid material can be workedupjn any desired manner, for example by agitating with hot water and dis: solving the soap stock which latter may be disposed of in any desired manner. Thev fullers earth,'when" that substance-is employed as a carrier for the alkali, does not, of course, dissolve "in water'du'ring the separation of the soap therefrom, and this fullers earth can again be impregnated with caustic alkali and re-used in the process. Thus the fullers earth or similar carriers can be reusedmany times.

.When other sol d chemically inert insoluble carriers are employed, the above mode of regenerating same for reuse, will-be satisfactory. When anhydrous soda or soap powder is used, the solid, material from which the oil has been removed can be sold as soap stock. -When pqwdei'ed abrasive Incas I such as kieselguhr or pumice is used as the carrier, the product can be usefully incorporated into scrubbing powders, etc.

'- In the process of refining, as herein de-, scribed, it is generally an object to remove the free fatty acids as completely as possible. However in some instance it would be suf;

I ficient to use far less than enough of the dry chemical and of water to accomplish this. Thus a highly coloredand highly odoriferous oil might be treated with only enough of the dry chemical and water, to

' somewhat brighten its color and remove some of its odorous substances while removin'giqnly half or less of its free fattyacid 1 content to cheaply improve a soap-making oil. In a modified form of theifgkpcess, I may add somewhat more waterfev'en continuing the addition of water after the break say while agitating. Thus I might use twice as much water-(more or less) as is needed for effecting the reaction. I can then settle ,and' decant or filter, if desired, although these operations at this stage are 'unnecessary. I can then suitably remove'the excess of water, e. g. by adding moreof the alkaline absorbent reagent followed bya short agitation and filtration.' Thi's modi-c fication may sometimes produce more bleaching or more complete removal of colloidal or suspended matters, but is not generally cussed the drying of the impregnated absorbent, e. g. fullers earth. When soap recommended.

In another modification of the'process, I can ad alternately several small amounts of water and of the dry chemical while agitating, until the desiredamount of purification .as been effected, and the oil may or may not be filtered, after each addition of chemical has had a chance to efi'ect the desired "purification. In this way, a minimum amount of chemical'would effect a maximum amountj of purification. Such a modification howevermight cost more in the way of addedhandling. Thus I may add the above stated amounts of chemical and water, (or smaller amounts, if preferred) in all,' but 7 these can be added 'in'several fractions, al-

once.

ternately, instead of being all .In a tparticular example'of the modification re erred to in thelast paragraph, I may add say one-half of one percent ofwater to cotton seed oil containing two peI;- cent fatty acids, stirthoroughly andadd say one-half of one percent of the dry chemical under agitation. Continue agitation for 10 minutes, then add another one-half perv added at cent of watefi/ followedby the addition of another one- If percent of dr chemical,

' all under continued agitation w ich is continned for say, another 15 to 30 minutes, then separate the resultant soap-stock.

I havereferred above to the use of caustic soda as the preferred neutralizing reagent.

Other alkalies such as the carbonates, oxides, and hydroxides of the alkali metals and alkaline earth metals, or ammonia gas, or salts ofv weak acids which give a baslc reaction, such as borates, silicates, or other agents capable of neutralizing free fatty acids, can be used. 4

H I have also referred to the use of strong solutions of alkali for impregnating the Y carrier materials. In some cases however, 7 relatively weak solutions or impregnation with only a small amount of alkaline solutions may be advisable. Thus I mayprepare dry chemical containing only 2 to 10%, more or less, of N aOH, which would be ver suitable when it is more especially desire to accomplish decolorization, precipitation of colloidal matters, etc., with only a small amount of neutralization of free fatty acids, as when treating oils in which 5 the fatty acid content is quite low. An example of t is is the treatment of cocoa fat from which it is desired to remove a large amount of coloring matters, colloidal suspended matters, etc. although the free fatty on powder is used as the absorbent, I may make a mixture of soap, alkali and waterin any desired proportions (e. g. 10: 8:5) and dry this mixture say in a vacuum drier, to eliminate the use of high temperatures. This dried material is then reduced to the desired state of fineness. I

.The advantages ofmy invention are: (m)

The yield ofneutral 011 from the refining steps is very greatlyincreased because the dry process practica y precludes the formation of emulsions. In the ordinary methodsof refining, this neutral oil loss is one of the greatest, and oftentimes the greatest item of refining cost, but b -my method this refining" loss is material y reduced. (b) The absorptionlosses in 'the bleaching and filtering step of the wet process methods are reduced to a fraction thereof because in my or carbons which absorb notable proportionsof oil,- thus eliminating these absorption losses and thereby also incmasing' manyfold the number of batches that may be run through the filter press before its capacity has been reached.- (a) Lower cost, (as compared with other 'puhficationpr'ocesses) \because of less labor and equipment required to carry on the process, and because of a 139 505, I have claime greater yield of neutral oil. (d) A further substantial reduction in cost and simplification of the whole process is effected by the decolorizing action taking place in the same stage with the neutralization of the free fatty acids. (6) A great saving in time is effected, since washing and subsequent settling are eliminated. (f) It becomes unnecessary to sub'ect the oil to high drying temperatures, t ereby insuring a better quality of oil, particularly when the same is to be used for edible purposes. (g) It practically precludes the formation of free fatty acids in the oil under treatment since the oil during processing does not encounter the usual washing and high heating steps. The neutral oil is practically completely freed of soap in one operation. (11) The workingup of the soap stock is simplified because of the practical absence of emulsions, which are always a source of large refining loss, and cost of handling. (j) The process presents especial value in the treatment of certain oils, such as castor oil, which, when subjected to the wet neutralizing methods, produce very troublesome emulsions or solutions, or both, in the refining kettle. My process completely eliminates the formation of such emulsions and solutions, 11

I have described in detail several embodt ments of my invention but it is to be vexpressly understood that I do not limit myself thereto or to the details related in connection with the specific embodiments described. I have also indulged in some theoretical discussions of what actually takes place in the practical use of my invention to more clearly elucidate the principles thereof. I may be mistaken about some of these theoretical considerations but I do know that when the steps of the process are carried out in the manner clearly indicated no difliculties will be encountered in practicing my methodand that substantial results, some of which have been referred to, will be achieved. Q

" In a concurrently filedapplication 122,- in particular, the aplication of this process to normally solid atty oils, and also the addition ofthe water after the addition of the dry chemical.

What I claim and desire to secure by Let ters Patent is:

1.-A rocess of refining normally liquid fatty 0i s from which the free fatty acids have not been removed, which comprises the steps of adding to and mixing with such oils adry, finely divided, alkali-impregnated reagent, and adding at any stage of the process suflicient water to promote a rapid neutralization of free fatty acids therein and to agglomerate-the resultant soap stock, the'amount of waterbeing insufficient to leave any substantial proportion of soap in I solution. I

2. A process ofmeutralizing acidity in a fatty oil emulsion containing a percentage of water which is only a minor fraction of the amount of the oil and of removing the water therefrom, and of removing colloidal substances and finely divided suspended matters therefrom, which comprises the steps of thoroughly distributing into. said fatty oil emulsion while carrying sufiicient water to promote reaction, a finely divided solid reagent comprising a solid material carrying a solid alkali intimately bonded thereto, which reagent is capable of abstracting water from such oil emulsion, in an amount suflicient to neutralize the fatty acid content of such fatty oil emulsion, whereby the oil is neutraling thoroughly incorporated therewith a dry neutralizing reagent to neutralizefree fattycolormg and resinous acids and to take u matter present in fiheoils, the amount of said dry neutralizing reagent being more than chemically equivalent to the free fatty acids in the oils, and the amount of the added water being insufiicient to leave any substantial amount of the soap in a liquid state in said oil.

fl. A process of relinim fatty oil which comprises the ste s of adding to fatty oil from which the rec fatty acids have not been removed, water and thereafter a substantially dry pulverulent intimate mixture of a solid material carrying an alkali, both in amounts sufficient to convert the free 'fatty acids into solid soap and to produce a free fatty acids, which comprises the step of adding to such anoilja small percentage of water and while below 140 F., and adding to said oil a quantity somewhat inexcess of that theoretically required 'of substantially dry fixed alkali carried. in a finely;

divlded solid agent to combine with thefree fatty acids present to produce soap/and a neutral oil and to absorbcoloring and resi25 inous matter. present in the oil.

6. In the purification of fatty oils containing substantial amounts of free fatty acids, the improvement which comprises combine with such free fatty acids.-

adding to such. oil while warm, a small percentage of water and a dry reagent comprising a dry solid vehicle carryinga dry alkali intimately bonded thereto, in such amounts as will convert the free fatty acids contained in the said fatty oil into a soap which is closely attached to said solid vehfcle, and thereafter separating the soap and insoluble material from the purified oil, the amount of water being not substantially greater than can be taken up by said dry reagent and the: reaction products formed.

7. In a process of refining a fatty oil containing free fatty acids, the ,steps which include forming a Warm mixture of such oil with a small percent of water, and adding a finely divided solid alkali-resistant material carrying dry fixed caustic alkali intimately bonded thereto, and agitating said mixture and material, and thereafter sepa-- such materials together, the amount of such dry reagent beingsufiicient,.in conjunction with the soap formed, to pick up substantially all the water present.

9. In a process of refining a fatty oil containing substantial quantities of free fatty acids the steps which include forming a warm'mixture of such oil with-an amount of water less than the amount of such fatty acids, and agitating same with a finely divided solid absorbing material carrying a dry fixed alkali in an amount sufiicient to r 10. A process of neutralizing acidity in an emulsion of a normally liquid fatty Oil and removing water, colloidal impurities and finely divided suspended matter therefrom,

. which comprises the step of adding a finely being sufiicient divided solid substance each particle of which is intimately associated with a dry agent capable of neutralizing such-acidity, the amount of such added material,'in conjunction with the reaction products formed, to leave the oil substantially anhydrous. w

11. In the purification of normally liquid fatty oil from which the free' fatty acids have not been removed, the herein described improvement which comprises adding to said oil while the latter contains a small amount of water, and while at a temperature at whic the oil is freely liquid but below 140 F., a reagent comprising a free solid alkali in a dry state intimately mixed with 'a dry finely divided solid material, then thoroughly mixing such oil andreagent together the total amount of Water present or "added being not above the amount which can be taken up by said solid reagent and react1on products, whereby the free fatty acids of the oil become substantially completely combined with the said alkali, and the waterbecomes absorbed by the solid. materials.

A 12. A process of refining cotton seed oil which comprises Well mixin crude cotton seed oil having a. normal ree fatty acid content 'with a dry intimate mixture containing a dry alkali intimately bonded to a finely divided solid material compatible therewith, and activating the reaction substances by adding at any'stage of the process, an

aqueous liquid non-injurious to the alkali,

capable of absorption by such solid materials and the reaction products.

.13. A process of refining fatty oils which comprises treating a fatty oil containlng free fatty acids with about 0.5 to 4% of water,-

and with aboutf2 to 10% of a dry reagent, such dry reagentcomprising a solid absorbent material carrying intimately incorporated therein, a caustic alkali, the amount ofsuch dry reagent and reaction products formed, beingalways sufficient to absorb the entire amount of water present in' the oil and added, and the caustic alkali in said dry reagent added being in excess over the amount theoretically necessary to neutralize all the free fatty acids present in said oil,

1 such water and dry reagent being added separately and in the order stated and the oil being at not above 140 F., during such treatment, and agitating the mixture.

.14. A process which comprises treating a normally liquid fatty oil containing free fatty acids, withabout 0.5 to 4% of water, and with not substantially above 5% of adry reagent, such drv reagent comprising a solid material carrying intimately incorporated therein, a caustic alkali; the amount of such dry reagent being always sufiicient, in

conjunction With the reaction products to absorb the entire amount of Water present in the oil and adde'l and thecaustic alkali in said dry reagen added being in excess over the amount thevretically necessary to neu tralize all the fre 7 fatty aci is present in said oil, such water and dry I'eagent being added separately but in any desired o1 der, and the oil being at not above 140-1f., during such treatment, and agitat Eng the mixture.

15. In a process f refining a fatty oil whose acid componeats have not previously been removi i, the step which comprises addin a sma.l percentage of water to such oil an thereafter adding thereto a dry finely divided solid material, the particles of which carry a dry alkali intimately bonded thereto, the total amount of water present at any to promote rapid neutralization and to sorbed by the solid material and solid reac-' tion products yielding an oil which is substantially anhydrous.

16. In a process of refining fatty oils containing freefatty acids and a small but substantial amount of water,-the step of adding to and mixing with such an oil a finely divided solid absorbent carrier material intimately associated with a dry alkali in an amount'suflicient to remove the impurities and all of the water from the oil.

In testimony whereofil have hereunto set my hand this 13th day of July, 1926.

' HENRY ODEEN. 

